One of the largest sources of uncertainty in radiocarbon dating stems from the sample pretreatment procedures used to minimize contamination. A major source of carbon contamination in charcoal from archaeological sites is humic substances carried by groundwater. Here we present a method, independent of 14C dating itself, to evaluate the effectiveness of the cleaning procedure of charcoal. Raman spectra of mixtures of humic substances (HS) and laboratory prepared charcoal indicate that Raman spectroscopy can be used as a semi-quantitative measure of the amount of humic substances associated with archaeological charcoal. Raman spectral analysis of archaeological charcoal samples subjected to different cleaning regimes supports this contention. Such measurements can provide quality control for charcoal preparation procedures and may assist in the interpretation of carbon-dating results.